CN108503358A - A kind of preparation method of superhigh temperature oxidation-resistant ceramic heater - Google Patents
A kind of preparation method of superhigh temperature oxidation-resistant ceramic heater Download PDFInfo
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- CN108503358A CN108503358A CN201810353932.2A CN201810353932A CN108503358A CN 108503358 A CN108503358 A CN 108503358A CN 201810353932 A CN201810353932 A CN 201810353932A CN 108503358 A CN108503358 A CN 108503358A
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Abstract
The invention discloses a kind of preparation methods of superhigh temperature oxidation-resistant ceramic heater, belong to heater preparing technical field.Ceramic heating element of the present invention is divided into two parts of internal layer and outer layer, doping component by the way that graphite to be used as to heater internal layer improves the capacity of heat transmission of heater internal layer, the rare earth metal of addition can improve ceramic resistor rate and elevated temperature strength, refine ceramic crystalline grain, creep rate is reduced, the present invention is combined with metallic bond between molybdenum and silicon in molybdenum disilicide used, then linked with covalent bond between silicon and silicon, for grey tetragonal crystal, SiO can be formed when the temperature of heating element is higher than 1700 DEG C2Protective film can condense at being 1710 DEG C in fusing point, with SiO2It is fused into melting drop, covering heater internal layer is made ceramic material obtained have good mechanical performance under superhigh temperature, had a extensive future to protect the high thermal conductivity material such as graphite synergistic effect that is not oxidized, and being filled mutually using silicon carbide and bentonite.
Description
Technical field
The invention discloses a kind of preparation methods of superhigh temperature oxidation-resistant ceramic heater, belong to fever Antibody Production Techniques neck
Domain.
Background technology
Ceramic heating element element is that electric heating element and ceramics are passed through high temperature sintering, a kind of fixed together manufactured fever member
Part so as to be overheated in setting value by temperature is constant, can have section according to the height regulation resistance size of body temperature
The features such as energy, safety, long lifespan.This heater does not shine at work, the flames of anger, anaerobic consumption, blow it is soft, have it is automatic
Temperature incubation function.PTC ceramics heater output power can arbitrarily adjust temperature at 800~1250 watts, and consumption that when work is unglazed has
Recloser, energy-efficient, power saving safety.The most of bathroom warm wind in the family of PTC ceramics heater purposes at present
Machine and some cubicles heat.Novel product-fireplace has been derived on the market being continuously improved now with consumer
Formula heater-simulation flame, generates warm wind at ceramic heat supply, builds warm American-European landscape（Power is up to 1800W）.Newly go out
A PTC ceramics heater appearance of product and common oil medium type heater likeness in form, but use enamel cooling fin.Feature is heat dissipation
Body, thin in profile have containment envelope, safe to use.Some the more advanced products used in present room have infrared ray
Remote control, timing shutdown, tumble such as automatically power off and heat at the functions, can be complete function.
The various key positions such as nose cone, nose of wing, the numbers of hot-side engine inner cavity of hypersonic aircraft or component are generally all
In the complicated Aerodynamic Heating higher than 1800 DEG C/couple of force conjunction or complicated burning situation.In order to ensure aerospace flight vehicle material
Performance can meet special Service Environment（Such as superhigh temperature, oxidation rigor condition）It is required that being badly in need of establishing and improving superhigh temperature etc.
The test method and technology of material property in extreme environment.The mechanics, anti-oxidant of the extreme environment of superhigh temperature oxidation at present
It is rarely reported with material properties experimental techniques such as thermal shock resistances, constrains the reality of superhigh temperature oxidation extreme environment material property
Test research.Wherein one of the main reasons is since the superhigh temperature heater of existing equipment is difficult to provide 1800 degree long-term and stably
Above oxidation environment.But there is an urgent need to be aoxidized in this superhigh temperature for the development of new and high technology and defence equipment construction at present
Material properties test under environment.Therefore, a kind of superhigh temperature oxidation-resistant ceramic heater is invented to heater preparing technical field
With positive effect.
Invention content
Present invention mainly solves the technical issues of, in current ceramic heating element zirconium oxide heater use when must be outer
Adding the heater of auxiliary or pre-heating device to be heated to 1000 DEG C or more can work, and graphite heater antioxygenic property is very poor,
It is only suitable for being applied to superhigh temperature vacuum or inert environments, the defect of the oxidation environment of superhigh temperature can not be applied to, provide one kind
The preparation method of superhigh temperature oxidation-resistant ceramic heater.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of superhigh temperature oxidation-resistant ceramic heater, it is characterised in that specifically preparation process is：
（1）40~50mL butyl titanates are added in the beaker equipped with 180~200mL ethylene glycol solutions, heat temperature raising, to beaker
Middle addition 30~35g citric acids start blender, are stirred, until citric acid is completely dissolved, obtain flaxen transparent molten
Liquid；
（2）20~25g neodymia and 30~35g lanthanas are dissolved in 200~250mL salpeter solutions, nitric acid rare earth gold is obtained
Belong to salting liquid, counts in parts by weight, 70~80 parts of above-mentioned flaxen clear solutions, 20~30 parts of nitric acid rare earth metal salts are molten
Liquid, 4~5 parts of calcium carbonate, 6~7 parts of lithium carbonates, 40~50 parts of zirconium oxide mixing are placed in water-bath, heat temperature raising, heat preservation, after
Continuous heat temperature raising, heat preservation obtain thick shape resin；
（3）Thick shape resin is put into coking furnace, nitrogen is passed through, heat temperature raising is put into pulverizer and crushes after keeping the temperature coking,
Resin particle is obtained, resin particle is placed in calcining furnace, is passed through air, heat temperature raising, pre-burning obtains ceramic powders, will be ceramic
Powder is mixed with poly-vinyl alcohol solution, is put into ball milling in ball mill, and sieving is used in combination deionized water to dilute ball milling slurry, is sent out
Hot volume surrounding slurry；
（4）Count in parts by weight, by 15~20 parts of silicon carbide, 10~12 parts of molybdenum disilicides, 20~30 parts of graphite powders, 10~15 parts
Bentonite and 10~20 parts of polyglycol solutions are fitted into ball milling in vibrator and obtain heater internal layer slurry；
（5）Fever volume surrounding slurry and heater internal layer slurry are injected into the mold for ceramic heating element, then by mold
It is placed in vacuum pre-burning in isostatic sintering stove, obtains vacuum pre-burning biscuit of ceramics；
（6）It continues up to state isostatic sintering stove and be passed through argon gas to furnace pressure and reaches certain initial pressure, start to warm up boosting
Sintering, last constant temperature and pressure are kept for a period of time, and superhigh temperature oxidation-resistant ceramic heater is obtained after cooled to room temperature.
Step（1）The mass fraction of the ethylene glycol solution is 25%, and beaker temperature is 80~100 DEG C after heat temperature raising.
Step（2）The salpeter solution mass fraction is 30%, and temperature is 80~85 DEG C after water-bath heat temperature raising, is protected
The warm time is 2~3h, and temperature is 130~150 DEG C after continuing heat temperature raising, and soaking time is 1~2h.
Step（3）Temperature is 230~250 DEG C after the heat temperature raising, and heat preservation scorch time is 30~35min, is crushed
Time is 3~4h, and heat temperature raising is 850~950 DEG C in calcining furnace, and burn-in time is 3~4h, poly-vinyl alcohol solution mass fraction
It is 5%, ceramic powders are 1 with poly-vinyl alcohol solution mixing quality ratio:2, Ball-milling Time is 10~15h, rule of being sieved in ball mill
Lattice are 200~300 mesh, are 2.2~2.5g/cm with deionized water dilution ball milling slurry density3。
Step（4）The mass fraction of the polyglycol solution is 10%, and control ball material mass ratio is 10:1, when ball milling
Between be 6~8h.
Step（5）The vacuum burn in step is：According to the speed of 40~50 DEG C/h, from room temperature to 280~300
DEG C, after keeping the temperature 2~3h, 400~550 DEG C are warming up to according still further to the speed of 60~70 DEG C/h, and keep the temperature 1h.
Step（6）It continues up to state isostatic sintering stove and be passed through initial pressure in argon gas to stove after the vacuum pre-burning and is
4~5kPa, increasing temperature and pressure sintering process are：1000 are warming up to by the heating rate of 300~500 DEG C/h to isostatic pressed sintering furnace
DEG C, 20~40min is kept the temperature, is then warming up to 1500 DEG C by the heating rate of 200~250 DEG C/h, keeps the temperature 20~40min, then press
The heating rate of 400~600 DEG C/h is warming up to 2000~2050 DEG C, 30~35min is kept the temperature, finally with the boosting of 6~8kPa/h
Speed increases pressure to 10~15kPa, and the last constant temperature and pressure retention time is 45~50min.
The beneficial effects of the invention are as follows：
（1）Calcium nitrate, magnesium nitrate, ethyl orthosilicate are scattered in absolute ethyl alcohol by the present invention to be hydrolyzed, and is stirred after polyvinyl alcohol is added
Dispersion is mixed, obtains mixed solution after adjusting pH, heated ageing obtains gel, and drying, sintering obtain calcium silicates magnesium powder
Body, using butyl titanate, ethylene glycol solution, citric acid as raw material, agitated dispersion obtains light yellow transparent solution, is added thereto
Nitric acid rare earth metal salt solution, calcium carbonate, lithium carbonate, zirconium oxide obtains thick shape resin by heat preservation complex reaction, by thick shape tree
Fat coking, crushing, sintering obtain ceramic powders, and ceramic powders are obtained fever volume surrounding slurry with poly-vinyl alcohol solution mixing defibrination
Material obtains heater internal layer slurry with zirconium oxide, silicon carbide, molybdenum disilicide, graphite powder, bentonite and polyethylene glycol mixing and ball milling
Material, enters mould, vacuum pre-burning obtains biscuit by slip casting, continues heating sintering and obtains superhigh temperature oxidation-resistant ceramic heater, this hair
Bright ceramic heating element is divided into two parts of internal layer and outer layer, and the doping component by the way that graphite to be used as to heater internal layer improves fever
The capacity of heat transmission of internal layer, makes ceramic heating element tentatively have certain high temperature with zirconium oxide fever volume surrounding as main component
The rare earth metal of oxidation resistance, addition can improve ceramic resistor rate and elevated temperature strength, refine ceramic crystalline grain, reduce creep rate,
Improve the high-temperature corrosion-resistance performance of ceramic heating element；
（2）The present invention is combined between molybdenum and silicon with metallic bond in molybdenum disilicide used, is then connected with covalent bond between silicon and silicon
Knot is grey tetragonal crystal, has good high-temperature oxidation resistance, the fine and close quartz of oxidizing atmosphere high temperature burning is in two silicon
Change and forms protection film layer on molybdenum surface, to prevent molybdenum disilicide continuous oxidation, the meeting when the temperature of heating element is higher than 1700 DEG C
Form SiO2Protective film can condense at being 1710 DEG C in fusing point, with SiO2Be fused into melting drop, covering heater internal layer from
And the high thermal conductivity material synergistic effect that is not oxidized, and being filled mutually using silicon carbide and bentonite such as protect graphite, make system
The ceramic material obtained has good mechanical performance under superhigh temperature, has a extensive future.
Specific implementation mode
40~50mL butyl titanates are added and are equipped in the beaker that 180~200mL mass fractions are 25% ethylene glycol solution,
80~100 DEG C are heated to, 30~35g citric acids are added into beaker, starts blender, with turning for 300~350r/min
Speed is stirred, until citric acid is completely dissolved, obtains flaxen clear solution；By 20~25g neodymia and 30~35g oxygen
Change lanthanum to be dissolved in the salpeter solution that 200~250mL mass fractions are 30%, obtains nitric acid rare earth metal salt solution, in parts by weight
Meter, by 70~80 parts of above-mentioned flaxen clear solutions, 20~30 parts of nitric acid rare earth metal salt solutions, 4~5 parts of calcium carbonate, 6~
7 parts of lithium carbonates, 40~50 parts of zirconium oxide mixing are placed in water-bath, are heated to 80~85 DEG C, are kept the temperature 2~3h, continue to add
Heat is warming up to 130~150 DEG C, keeps the temperature 1~2h, obtains thick shape resin；Thick shape resin is put into coking furnace, nitrogen is passed through, adds
Heat is warming up to 230~250 DEG C, after keeping the temperature 30~35min of coking, is put into 3~4h of crushing in pulverizer, obtains resin particle, will
Resin particle is placed in calcining furnace, is passed through air, is heated to 850~950 DEG C, and 3~4h of pre-burning obtains ceramic powders, will make pottery
The poly-vinyl alcohol solution that porcelain powder is 5% with mass fraction is 1 in mass ratio:2 mixing, are put into 10~15h of ball milling in ball mill,
200~300 mesh sieve is crossed, it is 2.2~2.5g/cm to be used in combination deionized water to dilute ball milling slurry to density3, obtain fever volume surrounding slurry
Material；It counts in parts by weight, by 15~20 parts of silicon carbide, 10~12 parts of molybdenum disilicides, 20~30 parts of graphite powders, 10~15 parts of swellings
The polyglycol solution that soil and 10~20 parts of mass fractions are 10% is fitted into vibrator, and control ball material mass ratio is 10:1,
6~8h of ball milling obtains heater internal layer slurry；Fever volume surrounding slurry and heater internal layer slurry are injected into for ceramics hair
In the mold of hot body, then mold is placed in vacuum pre-burning in isostatic sintering stove, first according to the speed of 40~50 DEG C/h, from room temperature
280~300 DEG C are warming up to, after keeping the temperature 2~3h, is warming up to 400~550 DEG C according still further to the speed of 60~70 DEG C/h, and keep the temperature 1h,
Obtain vacuum pre-burning biscuit of ceramics；It continues up that state isostatic sintering stove to be passed through argon gas to furnace pressure be 4~5kPa, and presses
The heating rate of 300~500 DEG C/h is warming up to 1000~1100 DEG C, keeps the temperature 20~40min, then presses the liter of 200~250 DEG C/h
Warm rate is warming up to 1500~1550 DEG C, keeps the temperature 20~40min, then 1900 are warming up to by the heating rate of 400~600 DEG C/h~
2000 DEG C, 30~35min is kept the temperature, pressure is finally increased to 10~15kPa with the rate of rise of 6~8kPa/h, constant temperature and pressure is protected
45~50min is held, superhigh temperature oxidation-resistant ceramic heater is obtained after cooled to room temperature.
Example 1
40mL butyl titanates are added and are equipped in the beaker that 180mL mass fractions are 25% ethylene glycol solution, are heated to 80
DEG C, 30g citric acids are added into beaker, starts blender, is stirred with the rotating speed of 300r/min, until citric acid is completely molten
Solution, obtains flaxen clear solution；It is molten that 20g neodymia and 30g lanthanas are dissolved in the nitric acid that 200mL mass fractions are 30%
In liquid, nitric acid rare earth metal salt solution is obtained, is counted in parts by weight, by 70 parts of above-mentioned flaxen clear solutions, 20 parts of nitric acid
Rare earth metal salt solutions, 4 parts of calcium carbonate, 6 parts of lithium carbonates, 40 parts of zirconium oxide mixing are placed in water-bath, are heated to 80 DEG C,
2h is kept the temperature, continues to be heated to 130 DEG C, keeps the temperature 1h, obtain thick shape resin；Thick shape resin is put into coking furnace, nitrogen is passed through
Gas is heated to 230 DEG C, after keeping the temperature coking 30min, is put into pulverizer and crushes 3h, obtain resin particle, by resin particle
It is placed in calcining furnace, is passed through air, be heated to 850 DEG C, pre-burning 3h obtains ceramic powders, by ceramic powders and mass fraction
Poly-vinyl alcohol solution for 5% is 1 in mass ratio:2 mixing, are put into ball milling 10h in ball mill, cross 200 mesh sieve, deionization is used in combination
It is 2.2g/cm that water, which dilutes ball milling slurry to density,3, obtain fever volume surrounding slurry；Count in parts by weight, by 15 parts of silicon carbide,
The polyglycol solution that 10 parts of molybdenum disilicides, 20 parts of graphite powders, 10 parts of bentonites and 10 parts of mass fractions are 10% is packed into vibrating ball
In grinding machine, control ball material mass ratio is 10:1, ball milling 6h obtain heater internal layer slurry；It will fever volume surrounding slurry and fever
Internal layer slurry is injected into the mold for ceramic heating element, then mold is placed in vacuum pre-burning in isostatic sintering stove, first
According to the speed of 40 DEG C/h, from room temperature to 280 DEG C, after keeping the temperature 2h, 400 DEG C are warming up to according still further to the speed of 60 DEG C/h, and
1h is kept the temperature, vacuum pre-burning biscuit of ceramics is obtained；Continue up state isostatic sintering stove be passed through argon gas to furnace pressure be 4kPa, and
1000 DEG C are warming up to by the heating rate of 300 DEG C/h, 20min is kept the temperature, is then warming up to 1500 by the heating rate of 200 DEG C/h
DEG C, 20min is kept the temperature, then 1900 DEG C are warming up to by the heating rate of 400 DEG C/h, keep the temperature 30min, finally with the boosting of 6kPa/h speed
Degree increases pressure to 10kPa, and constant temperature and pressure keeps 45min, and the fever of superhigh temperature oxidation-resistant ceramic is obtained after cooled to room temperature
Body.
Example 2
45mL butyl titanates are added and are equipped in the beaker that 190mL mass fractions are 25% ethylene glycol solution, are heated to 90
DEG C, 32g citric acids are added into beaker, starts blender, is stirred with the rotating speed of 320r/min, until citric acid is completely molten
Solution, obtains flaxen clear solution；It is molten that 22g neodymia and 32g lanthanas are dissolved in the nitric acid that 220mL mass fractions are 30%
In liquid, nitric acid rare earth metal salt solution is obtained, is counted in parts by weight, by 75 parts of above-mentioned flaxen clear solutions, 25 parts of nitric acid
Rare earth metal salt solutions, 4 parts of calcium carbonate, 6 parts of lithium carbonates, 45 parts of zirconium oxide mixing are placed in water-bath, are heated to 82 DEG C,
2.5h is kept the temperature, continues to be heated to 140 DEG C, keeps the temperature 1.5h, obtain thick shape resin；Thick shape resin is put into coking furnace, is led to
Enter nitrogen, be heated to 240 DEG C, after keeping the temperature coking 32min, is put into pulverizer and crushes 3.5h, obtain resin particle, will set
Fat particle is placed in calcining furnace, is passed through air, is heated to 900 DEG C, and pre-burning 3.5h obtains ceramic powders, by ceramic powders with
The poly-vinyl alcohol solution that mass fraction is 5% is 1 in mass ratio:2 mixing, are put into ball milling 12h in ball mill, cross 250 mesh sieve, and
It is 2.4g/cm with deionized water dilution ball milling slurry to density3, obtain fever volume surrounding slurry；It counts in parts by weight, by 17 parts
The polyglycol solution that silicon carbide, 11 parts of molybdenum disilicides, 25 parts of graphite powders, 12 parts of bentonites and 15 parts of mass fractions are 10% fills
Enter in vibrator, control ball material mass ratio is 10:1, ball milling 7h obtain heater internal layer slurry；It will fever volume surrounding slurry
Material and heater internal layer slurry are injected into the mold for ceramic heating element, then mold is placed in vacuum in isostatic sintering stove
Pre-burning, from room temperature to 290 DEG C, after keeping the temperature 2.5h, is warming up to first according to the speed of 45 DEG C/h according still further to the speed of 65 DEG C/h
500 DEG C, and 1h is kept the temperature, obtain vacuum pre-burning biscuit of ceramics；It continues up and states isostatic sintering stove and be passed through argon gas to furnace pressure
For 4kPa, and 1050 DEG C are warming up to by the heating rate of 400 DEG C/h, keep the temperature 30min, then press the heating rate liter of 220 DEG C/h
Temperature keeps the temperature 30min, then be warming up to 1950 DEG C by the heating rate of 500 DEG C/h, 32min is kept the temperature, finally with 7kPa/h to 1520 DEG C
The rate of rise increase pressure to 12kPa, constant temperature and pressure keeps 47min, and it is anti-oxidant to obtain superhigh temperature after cooled to room temperature
Ceramic heating element.
Example 3
50mL butyl titanates are added and are equipped in the beaker that 200mL mass fractions are 25% ethylene glycol solution, are heated to 100
DEG C, 35g citric acids are added into beaker, starts blender, is stirred with the rotating speed of 350r/min, until citric acid is completely molten
Solution, obtains flaxen clear solution；It is molten that 25g neodymia and 35g lanthanas are dissolved in the nitric acid that 250mL mass fractions are 30%
In liquid, nitric acid rare earth metal salt solution is obtained, is counted in parts by weight, by 80 parts of above-mentioned flaxen clear solutions, 30 parts of nitric acid
Rare earth metal salt solutions, 5 parts of calcium carbonate, 7 parts of lithium carbonates, 50 parts of zirconium oxide mixing are placed in water-bath, are heated to 85 DEG C,
3h is kept the temperature, continues to be heated to 150 DEG C, keeps the temperature 2h, obtain thick shape resin；Thick shape resin is put into coking furnace, nitrogen is passed through
Gas is heated to 250 DEG C, after keeping the temperature coking 35min, is put into pulverizer and crushes 4h, obtain resin particle, by resin particle
It is placed in calcining furnace, is passed through air, be heated to 950 DEG C, pre-burning 4h obtains ceramic powders, by ceramic powders and mass fraction
Poly-vinyl alcohol solution for 5% is 1 in mass ratio:2 mixing, are put into ball milling 15h in ball mill, cross 300 mesh sieve, deionization is used in combination
It is 2.5g/cm that water, which dilutes ball milling slurry to density,3, obtain fever volume surrounding slurry；Count in parts by weight, by 20 parts of silicon carbide,
The polyglycol solution that 12 parts of molybdenum disilicides, 30 parts of graphite powders, 15 parts of bentonites and 20 parts of mass fractions are 10% is packed into vibrating ball
In grinding machine, control ball material mass ratio is 10:1, ball milling 8h obtain heater internal layer slurry；It will fever volume surrounding slurry and fever
Internal layer slurry is injected into the mold for ceramic heating element, then mold is placed in vacuum pre-burning in isostatic sintering stove, first
According to the speed of 50 DEG C/h, from room temperature to 300 DEG C, after keeping the temperature 3h, 550 DEG C are warming up to according still further to the speed of 70 DEG C/h, and
1h is kept the temperature, vacuum pre-burning biscuit of ceramics is obtained；Continue up state isostatic sintering stove be passed through argon gas to furnace pressure be 5kPa, and
1100 DEG C are warming up to by the heating rate of 500 DEG C/h, 40min is kept the temperature, is then warming up to 1550 by the heating rate of 250 DEG C/h
DEG C, 40min is kept the temperature, then 2000 DEG C are warming up to by the heating rate of 600 DEG C/h, keep the temperature 35min, finally with the boosting of 8kPa/h speed
Degree increases pressure to 15kPa, and constant temperature and pressure keeps 50min, and the fever of superhigh temperature oxidation-resistant ceramic is obtained after cooled to room temperature
Body.
Comparative example
It is anti-to superhigh temperature produced by the present invention as a comparison case with the superhigh temperature oxidation-resistant ceramic heater of Shanghai company production
Superhigh temperature oxidation-resistant ceramic heater in oxide ceramic heater and comparative example carries out performance detection, testing result such as 1 institute of table
Show：
Test method：
Determination of conductive coefficients standard is detected by 17911 standards of GB/T；
Bending strength test is detected by 1965 standards of GB；
Heating rate test is detected using MELTING POINT TESTER；
Maximum operation (service) temperature is tested under oxidation environment：Ceramic heating element in example 1~3 and comparative example is placed on oxidation environment
Under, it heats up to it, measures its maximum temperature.
1 ceramic heating element performance measurement result of table
It is high according to the superhigh temperature oxidation-resistant ceramic heater thermal coefficient produced by the present invention of data among the above, at 2000 DEG C
Thermal coefficient reaches 65 W/mK under hot environment, and intensity is high, and intensity is high in a high temperauture environment, in an oxidizing environment highest
Temperature in use reaches 2600 DEG C, and antioxygenic property is good, has broad application prospects.
Claims (7)
1. a kind of preparation method of superhigh temperature oxidation-resistant ceramic heater, it is characterised in that specifically preparation process is：
（1）40~50mL butyl titanates are added in the beaker equipped with 180~200mL ethylene glycol solutions, heat temperature raising, to beaker
Middle addition 30~35g citric acids start blender, are stirred, until citric acid is completely dissolved, obtain flaxen transparent molten
Liquid；
（2）20~25g neodymia and 30~35g lanthanas are dissolved in 200~250mL salpeter solutions, nitric acid rare earth gold is obtained
Belong to salting liquid, counts in parts by weight, 70~80 parts of above-mentioned flaxen clear solutions, 20~30 parts of nitric acid rare earth metal salts are molten
Liquid, 4~5 parts of calcium carbonate, 6~7 parts of lithium carbonates, 40~50 parts of zirconium oxide mixing are placed in water-bath, heat temperature raising, heat preservation, after
Continuous heat temperature raising, heat preservation obtain thick shape resin；
（3）Thick shape resin is put into coking furnace, nitrogen is passed through, heat temperature raising is put into pulverizer and crushes after keeping the temperature coking,
Resin particle is obtained, resin particle is placed in calcining furnace, is passed through air, heat temperature raising, pre-burning obtains ceramic powders, will be ceramic
Powder is mixed with poly-vinyl alcohol solution, is put into ball milling in ball mill, and sieving is used in combination deionized water to dilute ball milling slurry, is sent out
Hot volume surrounding slurry；
（4）Count in parts by weight, by 15~20 parts of silicon carbide, 10~12 parts of molybdenum disilicides, 20~30 parts of graphite powders, 10~15 parts
Bentonite and 10~20 parts of polyglycol solutions are fitted into ball milling in vibrator and obtain heater internal layer slurry；
（5）Fever volume surrounding slurry and heater internal layer slurry are injected into the mold for ceramic heating element, then by mold
It is placed in vacuum pre-burning in isostatic sintering stove, obtains vacuum pre-burning biscuit of ceramics；
（6）It continues up to state isostatic sintering stove and be passed through argon gas to furnace pressure and reaches certain initial pressure, start to warm up boosting
Sintering, last constant temperature and pressure are kept for a period of time, and superhigh temperature oxidation-resistant ceramic heater is obtained after cooled to room temperature.
2. a kind of preparation method of superhigh temperature oxidation-resistant ceramic heater according to claim 1, it is characterised in that：
Step（1）The mass fraction of the ethylene glycol solution is 25%, and beaker temperature is 80~100 DEG C after heat temperature raising.
3. a kind of preparation method of superhigh temperature oxidation-resistant ceramic heater according to claim 1, it is characterised in that：
Step（2）The salpeter solution mass fraction is 30%, and temperature is 80~85 DEG C after water-bath heat temperature raising, when heat preservation
Between be 2~3h, continue heat temperature raising after temperature be 130~150 DEG C, soaking time be 1~2h.
4. a kind of preparation method of superhigh temperature oxidation-resistant ceramic heater according to claim 1, it is characterised in that：
Step（3）Temperature is 230~250 DEG C after the heat temperature raising, and heat preservation scorch time is 30~35min, grinding time
For 3~4h, heat temperature raising is 850~950 DEG C in calcining furnace, and burn-in time is 3~4h, and poly-vinyl alcohol solution mass fraction is
5%, ceramic powders are 1 with poly-vinyl alcohol solution mixing quality ratio:2, Ball-milling Time is 10~15h, be sieved specification in ball mill
It is 2.2~2.5g/cm with deionized water dilution ball milling slurry density for 200~300 mesh3。
5. a kind of preparation method of superhigh temperature oxidation-resistant ceramic heater according to claim 1, it is characterised in that：
Step（4）The mass fraction of the polyglycol solution is 10%, and control ball material mass ratio is 10:1, Ball-milling Time 6
~8h.
6. a kind of preparation method of superhigh temperature oxidation-resistant ceramic heater according to claim 1, it is characterised in that：
Step（5）The vacuum burn in step is：According to the speed of 40~50 DEG C/h, from room temperature to 280~300 DEG C,
After keeping the temperature 2~3h, 400~550 DEG C are warming up to according still further to the speed of 60~70 DEG C/h, and keep the temperature 1h.
7. a kind of preparation method of superhigh temperature oxidation-resistant ceramic heater according to claim 1, it is characterised in that：
Step（6）Continued up after the vacuum pre-burning state isostatic sintering stove be passed through in argon gas to stove initial pressure be 4~
5kPa, increasing temperature and pressure sintering process are：1000 DEG C are warming up to by the heating rate of 300~500 DEG C/h to isostatic pressed sintering furnace, is protected
20~40min of temperature is then warming up to 1500 DEG C by the heating rate of 200~250 DEG C/h, keeps the temperature 20~40min, then by 400~
The heating rate of 600 DEG C/h is warming up to 2000~2050 DEG C, 30~35min is kept the temperature, finally with the rate of rise liter of 6~8kPa/h
For high pressure to 10~15kPa, the last constant temperature and pressure retention time is 45~50min.
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| CN110407588A (en) * | 2019-06-21 | 2019-11-05 | 杨晓军 | A kind of preparation method coating far infrared glaze layer stuffing sand |
| CN113292334A (en) * | 2021-05-12 | 2021-08-24 | 张建军 | High-temperature electronic superconductor and preparation method thereof |
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